CN101948133A - Method for co-producing sodium stannate and stannic oxide by solder removing liquid - Google Patents
Method for co-producing sodium stannate and stannic oxide by solder removing liquid Download PDFInfo
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- CN101948133A CN101948133A CN 201010521861 CN201010521861A CN101948133A CN 101948133 A CN101948133 A CN 101948133A CN 201010521861 CN201010521861 CN 201010521861 CN 201010521861 A CN201010521861 A CN 201010521861A CN 101948133 A CN101948133 A CN 101948133A
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- Prior art keywords
- acid
- sodium stannate
- filter cake
- tindioxide
- stripping liquid
- Prior art date
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Abstract
The invention discloses a method for co-producing sodium stannate and stannic oxide by solder removing liquid, comprising the following steps: separating tin in the solder removing liquid, recovering copper, transforming copper into sodium stannate, preparing sodium stannate and preparing stannic oxide. The method of the invention features in low processing cost, simple technical process and device structure, and high product purity and can prepare sodium stannate and stannic oxide.
Description
Technical field
The present invention relates to a kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide, particularly a kind of method of utilizing non-fluoridate type printed board tin stripping liquid coproduction sodium stannate and tindioxide.
Background technology
The PCB(printed circuit board) enterprise is a generation industry that liquid/solid trade waste quantity is bigger, a class I liquid I waste (abbreviating waste liquid as) that is produced, be the scrapping or produce when changing cylinder of liquid in the work nest of each operation, be characterized in Pollutant levels height, many, the complicated component of type.Moving back tin is the operation that produces the wastewater flow rate maximum in the PCB enterprise, the tin stripping liquid heavy metal content height that is produced (tin copper content can reach more than the 100g/L), the pollution index height, and free acid acidity is big, complicated component, generally contain multiple compositions such as acids (nitric acid, sulfuric acid, hydrochloric acid and other organic acid), promotor, tensio-active agent, oxynitride inhibitor, heavy metal complexing agent, copper inhibitor, be difficult to handle with ordinary method.How effectively to handle a difficult problem that waste tin stripper has become PCB enterprise to be faced.
Application number is that 200910301263.5 Chinese patent application discloses a kind of recovery method of tin in tin-stripping, adopt the sodium carbonate solution neutralization to move back the tin waste liquid, add alkali again and under 102 ℃ of-115 ℃ of temperature, be converted into sodium stannate, after the filtration, in filtrate, feed carbonic acid gas, make sodium stannate be converted into metastannic acid, after the filtration, produce tindioxide through washing, calcining.This method does not adopt distillation to reclaim nitric acid, need a large amount of use yellow soda ash go in and nitric acid, increased production cost, simultaneously with SODIUMNITRATE (containing some other soluble impurity) waste water of new increase, this part waste water needs further to handle, and has further increased production cost.This method feeds carbonic acid gas sodium stannate is transformed back metastannic acid, is sintered into tindioxide again, and the finished product are tindioxide only, has lost to separate the chance that obtains sodium stannate.
Application number is that 200810065305.5 Chinese patent application discloses a kind of method of utilizing circuit board tin-stripping wastewater to prepare sodium stannate, method to tin-stripping wastewater neutralization precipitation gained tin mud employing high-temperature roasting is converted into the resolvability sodium stannate with insoluble β-stannic acid, inferior stannic acid.This method need use yellow soda ash to go neutralization to move back the tin waste liquid equally, has increased production cost; Adopt the method for high-temperature fusion that β-stannic acid is transformed, need to adopt high-temperature fusion equipment, this device structure is complicated, and the equipment material requirement is special, operation is complicated, risk level is high, and cost is higher; Adopt counter-current lixiviate sodium stannate, again through press filtration, concentrate, filter, wash product, contain relatively large sodium hydroxide in the sodium stannate that concentration process obtains, be through the washing of the sodium hydroxide solution of 10% left and right sides concentration, could obtain qualified product, complex technical process.
Summary of the invention
The objective of the invention is to overcome the deficiency of tin stripping liquid processing cost height, technological process and device structure complexity in the prior art, a kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide is provided.This method processing cost is low, technological process and device structure is simple, product purity is high, can prepare sodium stannate and tindioxide simultaneously.
For achieving the above object, the technical solution adopted for the present invention to solve the technical problems is:
A kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide may further comprise the steps:
A, with tin stripping liquid at temperature 50-70 ℃, pressure 0.1 * 1.03 * 10
5-0.4 * 1.03 * 10
5Carry out underpressure distillation under the Pa and reclaim nitric acid, add ionogen in steaming surplus liquid, electrolytical dosage is the 20-60g/L tin stripping liquid, treat that sedimentation is finished after, press filtration, filter cake press dry after washing;
B, the filtrate that obtains in the steps A and washings are added the alkali neutralization, control pH value of solution value adds sodium sulfide solution to precipitating not regeneration again at 6-8, filters, and filter cake is a cupric sulfide, and filtrate is sent to Sewage treatment systems;
C, with in the steps A to filter cake send into reactor, adding is the solid alkali of 1:2-1:3.5 with the filter cake mol ratio, under agitation be warming up to 98-105 ℃, insulation 1-2h makes β-metastannic acid and α-metastannic acid be converted into sodium stannate, and adding is the water of 1:3-1:5 with the sodium stannate mass ratio again, stir, constant temperature 2-4h under 96-100 ℃ of temperature filters, and filter cake is sent to the iron recovery system;
D, with among the step C to filtrate heating be concentrated into crystal and occurred after, stop heating, natural cooling crystallization is filtered, dry cake obtains sodium stannate;
E, the back is mother liquid obtained to add the acid neutralization with filtering among the step D, through centrifugal, and press filtration, washing obtains metastannic acid, and metastannic acid at 200-400 ℃ of roasting temperature, is obtained tindioxide.
As optimal way, in the described steps A, ionogen is selected from Na
2SO
4, Na
3PO
4, K
2SO
4Or K
3PO
4In one or more.
As optimal way, among the described step C, alkali is selected from NaOH, KOH, Na
2CO
3Or NH
3H
2Among the O one or more.
As optimal way, in the described step e, acid is selected from one or more in hydrochloric acid, sulfuric acid, carbonic acid or the phosphoric acid.
The tin stripping liquid of the present invention after nitric acid is reclaimed in underpressure distillation, sedimentation takes place after adding ionogen, copper retains in the solution with ionic state, and the small part copper that adsorbs in the filter residue can reclaim through washing, and a small amount of remaining copper is converted into insoluble copper hydroxide and separates in the step that sodium stannate transforms.The filter residue that settles down is beyond deleading, aluminium exist with the acid salt form after the alkali conversion, and other impurity conversion is insoluble oxyhydroxide, is adding flooding Na
2SnO
4After filtration procedure insoluble oxyhydroxide can be removed, utilize the gluey characteristics of oxyhydroxide simultaneously, can effectively adsorb and remove part aluminium, silicate impurity.
Na of the present invention
2SnO
4With SnO
2The analysis indexes of product sees Table 1,2.
Table 1 Na
2SnO
4The analysis indexes of product
Table 2 SnO
2The analysis indexes of product
The present invention adopts underpressure distillation to reclaim nitric acid earlier, carries out potential of hydrogen again and regulates, and has both reclaimed nitric acid, realizes recycling, has reduced production cost, avoids again producing a large amount of SODIUMNITRATE waste water, has reduced discharge of wastewater and environmental pollution.
The present invention adopts solid NaOH and metastannic acid reaction, and controlled temperature is converted into the solubility stannate at 95-105 ℃ with higher transformation efficiency, has avoided high-temperature operation, has reduced the usage quantity of alkali, and technology and device structure are simple, have reduced production cost.The present invention adopts the flooding sodium stannate, has avoided adopting that the lixiviate of alkali strong solution brings at finished product Na
2SnO
4In the problem of remaining a large amount of NaOH, can disposablely reach Na
2SnO
4Commercially available specification of quality.
The present invention will produce Na
2SnO
4After mother liquor with after the acid neutralization, through centrifugal, calcining, grinding, washing, drying, produce SnO
2, solved the problem that mother liquor stockpiles, obtained SnO simultaneously again
2The fine chemistry product has fully been realized the resource utilization of useful component, has avoided the pollution to environment.
Beneficial effect of the present invention is: processing cost of the present invention is low, technological process and device structure is simple, product purity is high, can prepare sodium stannate and tindioxide simultaneously.
Embodiment
Disclosed all features in this specification sheets, or the step in disclosed all methods or the process except mutually exclusive feature and/or step, all can make up by any way.
Get five kinds of different tin stripping liquids, its moiety sees Table 3.
Main component content in table 3 water sample
Embodiment 1: a kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide may further comprise the steps: A, with tin stripping liquid at 70 ℃ of temperature, pressure 0.1 * 1.03 * 10
5Under carry out underpressure distillation and reclaim nitric acid, in steaming surplus liquid, add Na
2SO
4, electrolytical dosage is the 30g/L tin stripping liquid, treat that sedimentation is finished after, press filtration, filter cake through the washing after press dry;
B, the filtrate that obtains in the steps A and washings are added the alkali neutralization, control pH value of solution value adds sodium sulfide solution to precipitating not regeneration again at 6-8, filters, and filter cake is a cupric sulfide, and filtrate is sent to Sewage treatment systems;
C, with in the steps A to filter cake send into reactor, adding is the solid NaOH of 1:2 with the filter cake mol ratio, under agitation be warming up to 98 ℃, insulation 2h makes β-metastannic acid and α-metastannic acid be converted into sodium stannate, and adding is the water of 1:3 with the sodium stannate mass ratio again, stir, constant temperature 4h under 96 ℃ of temperature filters, and filter cake is sent to the iron recovery system;
D, with among the step C to filtrate heating be concentrated into crystal and occurred after, stop heating, natural cooling crystallization is filtered, dry cake obtains sodium stannate;
E, the back is mother liquid obtained to add the acid neutralization with filtering among the step D, through centrifugal, and press filtration, washing obtains metastannic acid, and metastannic acid at 300 ℃ of roasting temperatures, is obtained tindioxide.
Embodiment 2: a kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide may further comprise the steps:
A, with tin stripping liquid at 50 ℃ of temperature, pressure 0.4 * 1.03 * 10
5Carry out underpressure distillation under the Pa and reclaim nitric acid, in steaming surplus liquid, add Na
3PO
4, Na
3PO
4Dosage be the 60g/L tin stripping liquid, treat that sedimentation is finished after, press filtration, filter cake through the washing after press dry;
B, the filtrate that obtains in the steps A and washings are added the alkali neutralization, control pH value of solution value adds sodium sulfide solution to precipitating not regeneration again at 6-8, filters, and filter cake is a cupric sulfide, and filtrate is sent to Sewage treatment systems;
C, with in the steps A to filter cake send into reactor, adding is the solid KOH of 1:3.5 with the filter cake mol ratio, under agitation be warming up to 105 ℃, insulation 1h makes β-metastannic acid and α-metastannic acid be converted into sodium stannate, and adding is the water of 1:5 with the sodium stannate mass ratio again, stir, constant temperature 2h under 100 ℃ of temperature filters, and filter cake is sent to the iron recovery system;
D, with among the step C to filtrate heating be concentrated into crystal and occurred after, stop heating, natural cooling crystallization is filtered, dry cake obtains sodium stannate;
E, the back is mother liquid obtained to add the acid neutralization with filtering among the step D, through centrifugal, and press filtration, washing obtains metastannic acid, and metastannic acid at 200 ℃ of roasting temperatures, is obtained tindioxide.
Embodiment 3: a kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide may further comprise the steps:
A, with tin stripping liquid at 60 ℃ of temperature, pressure 0.3 * 1.03 * 10
5Carry out underpressure distillation under the Pa and reclaim nitric acid, in steaming surplus liquid, add K
2SO
4, K
2SO
4Dosage be the 40g/L tin stripping liquid, treat that sedimentation is finished after, press filtration, filter cake through the washing after press dry;
B, the filtrate that obtains in the steps A and washings are added the alkali neutralization, control pH value of solution value adds sodium sulfide solution to precipitating not regeneration again at 6-8, filters, and filter cake is a cupric sulfide, and filtrate is sent to Sewage treatment systems;
C, with in the steps A to filter cake send into reactor, add with the filter cake mol ratio be the solid NH of 1:3
3H
2O under agitation is warming up to 100 ℃, and insulation 1.5h makes β-metastannic acid and α-metastannic acid be converted into sodium stannate, and adding is the water of 1:4 with the sodium stannate mass ratio again, stirs, and constant temperature 3h under 98 ℃ of temperature filters, and filter cake is sent to the iron recovery system;
D, with among the step C to filtrate heating be concentrated into crystal and occurred after, stop heating, natural cooling crystallization is filtered, dry cake obtains sodium stannate;
E, the back is mother liquid obtained to add the acid neutralization with filtering among the step D, through centrifugal, and press filtration, washing obtains metastannic acid, and metastannic acid at 400 ℃ of roasting temperatures, is obtained tindioxide.
Embodiment 4: a kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide may further comprise the steps:
A, with tin stripping liquid at 65 ℃ of temperature, pressure 0.3 * 1.03 * 10
5Carry out underpressure distillation under the Pa and reclaim nitric acid, in steaming surplus liquid, add K
3PO
4, K
3PO
4Dosage be the 50g/L tin stripping liquid, treat that sedimentation is finished after, press filtration, filter cake through the washing after press dry;
B, the filtrate that obtains in the steps A and washings are added the alkali neutralization, control pH value of solution value adds sodium sulfide solution to precipitating not regeneration again at 6-8, filters, and filter cake is a cupric sulfide, and filtrate is sent to Sewage treatment systems;
C, with in the steps A to filter cake send into reactor, adding is the solid NaOH of 1:3 with the filter cake mol ratio, under agitation be warming up to 102 ℃, insulation 2h makes β-metastannic acid and α-metastannic acid be converted into sodium stannate, and adding is the water of 1:4 with the sodium stannate mass ratio again, stir, constant temperature 3h under 100 ℃ of temperature filters, and filter cake is sent to the iron recovery system;
D, with among the step C to filtrate heating be concentrated into crystal and occurred after, stop heating, natural cooling crystallization is filtered, dry cake obtains sodium stannate;
E, the back is mother liquid obtained to add the acid neutralization with filtering among the step D, through centrifugal, and press filtration, washing obtains metastannic acid, and metastannic acid at 350 ℃ of roasting temperatures, is obtained tindioxide.
Embodiment 5: step is with embodiment 4.
Add among the embodiment 1-5 that the rate of descent of tin sees Table 4 behind the ionogen.
The rate of descent of tin behind the table 4 adding ionogen
The rate of descent of tin all is higher than 99.5% among the embodiment 1-5, and the separation rate height of tin has fully reclaimed valuable tin element in the tin stripping liquid, has remarkable economic efficiency and social benefit.
The present invention is not limited to aforesaid embodiment.The present invention expands to any new feature or any new combination that discloses in this manual, and the arbitrary new method that discloses or step or any new combination of process.
Claims (4)
1. method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide is characterized in that may further comprise the steps:
A, with tin stripping liquid at temperature 50-70 ℃, pressure 0.1 * 1.03 * 10
5-0.4 * 1.03 * 10
5Carry out underpressure distillation under the Pa and reclaim nitric acid, add ionogen in steaming surplus liquid, electrolytical dosage is the 20-60g/L tin stripping liquid, treat that sedimentation is finished after, press filtration, filter cake press dry after washing;
B, the filtrate that obtains in the steps A and washings are added the alkali neutralization, control pH value of solution value adds sodium sulfide solution to precipitating not regeneration again at 6-8, filters, and filter cake is a cupric sulfide, and filtrate is sent to Sewage treatment systems;
C, with in the steps A to filter cake send into reactor, adding is the solid alkali of 1:2-1:3.5 with the filter cake mol ratio, under agitation be warming up to 98-105 ℃, insulation 1-2h makes β-metastannic acid and α-metastannic acid be converted into sodium stannate, and adding is the water of 1:3-1:5 with the sodium stannate mass ratio again, stir, constant temperature 2-4h under 96-100 ℃ of temperature filters, and filter cake is sent to the iron recovery system;
D, with among the step C to filtrate heating be concentrated into crystal and occurred after, stop heating, natural cooling crystallization is filtered, dry cake obtains sodium stannate;
E, the back is mother liquid obtained to add the acid neutralization with filtering among the step D, through centrifugal, and press filtration, washing obtains metastannic acid, and metastannic acid at 200-400 ℃ of roasting temperature, is obtained tindioxide.
2. a kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide as claimed in claim 1, it is characterized in that: in the described steps A, ionogen is selected from Na
2SO
4, Na
3PO
4, K
2SO
4Or K
3PO
4In one or more.
3. a kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide as claimed in claim 1 is characterized in that: among the described step C, alkali is selected from NaOH, KOH, Na
2CO
3Or NH
3H
2Among the O one or more.
4. a kind of method of utilizing tin stripping liquid coproduction sodium stannate and tindioxide as claimed in claim 1 is characterized in that: in the described step e, acid is selected from one or more in hydrochloric acid, sulfuric acid, carbonic acid or the phosphoric acid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010521861.6A CN101948133B (en) | 2010-10-28 | 2010-10-28 | Method for co-producing sodium stannate and stannic oxide by solder removing liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010521861.6A CN101948133B (en) | 2010-10-28 | 2010-10-28 | Method for co-producing sodium stannate and stannic oxide by solder removing liquid |
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| CN101948133B CN101948133B (en) | 2014-08-06 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923764A (en) * | 2012-10-25 | 2013-02-13 | 中南大学 | Method for preparing sodium stannate from stannic oxide and sodium salt in reduction roasting manner |
| CN104152701A (en) * | 2014-08-18 | 2014-11-19 | 汨罗市绿岩金属有限公司 | Method for recycling tin from coarse tin refining slag |
| CN104894599A (en) * | 2015-06-23 | 2015-09-09 | 成都虹华环保科技股份有限公司 | Recycling process of tin-removing waste liquid |
| CN104986892A (en) * | 2015-07-02 | 2015-10-21 | 清远市新绿环境技术有限公司 | Tin stripping waste liquid treating method |
| CN105293454A (en) * | 2015-10-27 | 2016-02-03 | 盛隆资源再生（无锡）有限公司 | Method for preparing dilute nitric acid, sponge tin and polymeric aluminum through spent tin-fading liquid |
| WO2016184249A1 (en) * | 2015-05-21 | 2016-11-24 | 成都虹华环保科技股份有限公司 | Nitric acid tin-stripping liquid treatment system |
| CN108070720A (en) * | 2017-11-10 | 2018-05-25 | 河海大学 | A kind of comprehensive recovering process of tin removal waste liquor |
| CN109536982A (en) * | 2018-12-27 | 2019-03-29 | 广东先导稀材股份有限公司 | Preparation method of nano tin dioxide |
| CN109633076A (en) * | 2018-12-10 | 2019-04-16 | 广东省佛山地质局(广东省佛山地质灾害应急抢险技术中心) | The measuring method of Theil indices in the preprocess method and tin stripper of tin stripper |
| CN115232985A (en) * | 2022-07-01 | 2022-10-25 | 清远市中宇环保实业有限公司 | Novel alkaline leaching-crystallization preparation process for tin in tin-containing sludge |
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| CN1530466A (en) * | 2003-03-11 | 2004-09-22 | 湖南高奇实业有限公司 | Recovery of tin from waste liquid of tin and lead |
| CN1569644A (en) * | 2004-04-30 | 2005-01-26 | 深圳市危险废物处理站 | Method for preparing barium stannate trihydrate using stannum in waste tin stripper |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923764B (en) * | 2012-10-25 | 2014-07-30 | 中南大学 | Method for preparing sodium stannate from stannic oxide and sodium salt in reduction roasting manner |
| CN102923764A (en) * | 2012-10-25 | 2013-02-13 | 中南大学 | Method for preparing sodium stannate from stannic oxide and sodium salt in reduction roasting manner |
| CN104152701A (en) * | 2014-08-18 | 2014-11-19 | 汨罗市绿岩金属有限公司 | Method for recycling tin from coarse tin refining slag |
| CN104152701B (en) * | 2014-08-18 | 2017-06-13 | 汨罗市绿岩金属有限公司 | The method that tin is reclaimed from tin refinement slag |
| WO2016184249A1 (en) * | 2015-05-21 | 2016-11-24 | 成都虹华环保科技股份有限公司 | Nitric acid tin-stripping liquid treatment system |
| CN104894599A (en) * | 2015-06-23 | 2015-09-09 | 成都虹华环保科技股份有限公司 | Recycling process of tin-removing waste liquid |
| WO2016206418A1 (en) * | 2015-06-23 | 2016-12-29 | 成都虹华环保科技股份有限公司 | Recycling and reusing process for spent tin stripper solution |
| CN104986892A (en) * | 2015-07-02 | 2015-10-21 | 清远市新绿环境技术有限公司 | Tin stripping waste liquid treating method |
| CN105293454A (en) * | 2015-10-27 | 2016-02-03 | 盛隆资源再生（无锡）有限公司 | Method for preparing dilute nitric acid, sponge tin and polymeric aluminum through spent tin-fading liquid |
| CN108070720A (en) * | 2017-11-10 | 2018-05-25 | 河海大学 | A kind of comprehensive recovering process of tin removal waste liquor |
| CN109633076A (en) * | 2018-12-10 | 2019-04-16 | 广东省佛山地质局(广东省佛山地质灾害应急抢险技术中心) | The measuring method of Theil indices in the preprocess method and tin stripper of tin stripper |
| CN109536982A (en) * | 2018-12-27 | 2019-03-29 | 广东先导稀材股份有限公司 | Preparation method of nano tin dioxide |
| CN109536982B (en) * | 2018-12-27 | 2021-04-13 | 广东先导稀材股份有限公司 | Preparation method of nano tin dioxide |
| CN115232985A (en) * | 2022-07-01 | 2022-10-25 | 清远市中宇环保实业有限公司 | Novel alkaline leaching-crystallization preparation process for tin in tin-containing sludge |
| CN115232985B (en) * | 2022-07-01 | 2024-01-16 | 清远市中宇环保实业有限公司 | Alkaline leaching-crystallization preparation process of tin in tin-containing sludge |
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